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標題: 磺酸化導電高分子/奈米碳管複合材料之製備與特性研究
Preparation and Characterization of Sulfonated Conducting Polymer/Carbon Nanotube Composites
作者: 林彥文
Lin, Yen-Wen
關鍵字: Sulfonated Conducting Polymer
Carbon Nanotube
出版社: 材料科學與工程學系所
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摘要: 本研究藉由溶液混合方式於水溶液環境下結合磺酸化聚苯胺與羧酸化多壁奈米碳管,並製備出具水溶特性之核殼管狀結構複合物。傅立葉轉換紅外光譜儀、拉曼光譜儀、紫外可見光譜儀、化學分析能譜儀、場發射掃瞄式電子顯微鏡和高解析度穿透式電子顯微鏡被使用來觀察磺酸化聚苯胺/羧酸化多壁奈米碳管複合物的形態與結構。其中,由拉曼、紫外可見光譜儀及化學分析能譜儀的分析結果中可得知磺酸化聚苯胺結構中的C–N+與羧酸化多壁奈米碳管的COO-間存在著靜電作用力。而羧酸化多壁奈米碳管的添加可補強磺酸化聚苯胺的熱穩定特性。當複合物中含有3 wt%羧酸化多壁奈米碳管時,其室溫下的導電度數值為磺酸化聚苯胺樣品的16倍之高,此導電數值的變化顯現出只要少量的羧酸化多壁奈米碳管,即可在複合物結構中構建良好的網狀導電通路,並藉此提升磺酸化聚苯胺/羧酸化多壁奈米碳管複合物的導電性質。另外,相似的溶液混合方式也應用於水溶性磺酸化聚吡咯/羧酸化多壁奈米碳管複合物之製備。 另一方面,磺酸化聚苯胺/羧酸化多壁奈米碳管複合物的電化學特性則以循環伏安法及電化學交流阻抗光譜法加以研究。研究結果顯示當羧酸化多壁奈米碳管存在於磺酸化聚苯胺基材中時,可增加磺酸化聚苯胺/羧酸化多壁奈米碳管複合薄膜的電化學活性,並增進氧化還原反應時的電子傳遞行為。再者,羧酸化多壁奈米碳管的存在同時也使得電化學反應的活性區域增加,並加快原本磺酸化聚苯胺上的電子傳遞。而藉由場發射掃瞄式電子顯微鏡和原子力顯微鏡所進行的表面形態分析結果,可證實複合薄膜表面分佈著分散良好的管狀結構,而相對粗糙的複合薄膜表面則提供了電極工作時所需要的反應面積。因此,表面形貌上的差異佐證了磺酸化聚苯胺/羧酸化多壁奈米碳管複合薄膜具有高電化學特性的原因。 研究中同時利用電紡絲技術成功地製備出磺酸化聚苯胺/聚氧化乙烯電紡絲纖維產物,其中欲獲得形態良好之電紡絲纖維的關鍵參數取決於電紡絲液體的黏度特性。研究結果顯示磺酸化聚苯胺的存在使得電紡絲液體所帶的電荷密度增加,因此可得到平均纖維直徑較小之電紡絲纖維產物。當磺酸化聚苯胺/聚氧化乙烯的重量比為0.33時,所得電紡絲纖維產物之導電度數值高於磺酸化聚苯胺/聚氧化乙烯重量比為0.2時之5倍以上。此外,電紡絲技術可輕易將羧酸化多壁奈米碳管複合至磺酸化聚苯胺/聚氧化乙烯電紡絲纖維中。高解析度穿透式電子顯微鏡影像證實羧酸化多壁奈米碳管確實存在於電紡絲纖維中,並平行排列於電紡絲纖維的軸向。而量測結果顯示電紡絲纖維的導電度數值隨著羧酸化多壁奈米碳管含量的增加而呈現上升的趨勢。
The water-soluble sulfonated polyaniline (SPANI)/carboxylic groups containing multi-walled carbon nanotube (c-MWCNT) composites with core-shell tubular structure have been prepared by solution mixing of c-MWCNT and SPANI aqueous colloids. Fourier-transform infrared spectroscopy, Raman spectroscopy, ultraviolet-visible (UV-Vis) absorption spectroscopy, X-ray photoelectron spectroscopy (XPS), field- emission scanning (SEM) and high-resolution transmission electron microscopy (HRTEM) were used to characterize their structure and morphology of composites. The results of Raman, UV-Vis and XPS spectra revealed the presence of electrostatic interaction between the C-N+ species of the SPANI and the COO- species of the c-MWCNTs. The addition of c-MWCNTs can improve the thermal stability of SPANI specimens. The conductivity of 3 wt% SPANI/c-MWCNT composites at room temperature is sixteen times higher than that of SPANI. The above results demonstrate that the addition of a small number of c-MWCNTs into SPANI matrix can efficiently form a conducting network in the well dispersed composites, thus increasing the electrical properties of the composites. In addition, similar methodology has been applied to fabricate the water-soluble sulfonated polypyrrole (SPPy)/c-MWCNT composites by aqueous mixing of c-MWCNT dispersions and SPPy colloids. The electrochemical performances of these SPANI/c-MWCNT composites have been investigated using cyclic voltammetry and electrochemical impedance spectro- scopy. The incorporation of the c-MWCNTs to SAPNI increases the electrochemical activity of SPANI/c-MWCNT composite films and promotes the electron transfer of the redox processes. Furthermore, the presence of c-MWCNTs also leads to more active sites for electrochemical reactions and a faster electron transfer than pure SAPNI. In addition, the morphology of SPANI/c-MWCNT composites measured by SEM and atomic force microscopy indicates the presence of well-distributed tubular structures that are individually coated with ED-SPANI on the surface of composite films. The relatively rough topography of composite films would provide a large surface area for electrolyte access. Therefore, it is expected that the difference in the structure of the composite films can result in high electrochemical properties of the electrodes constructed from these composite films. The electrospinning process has been successfully used to fabricate ultrafine fibers consisting of the mixture of SPANI and poly(ethylene oxide) (PEO). The key factor of fiber formation with uniform size of fibers were dependent on the solution viscosity. The SEM images showed that the average diameter of SPANI/PEO electrospun fibers were evidently decreased with increasing loading of SPANI content. This trendency may be attributed to the increase in the net charge density of the solution with the presence of SPANI, which favors the formation of thin fibers. The conductivity of SPANI/PEO electrospun fibers fabricated with the weight ratio of SPANI/PEO at 0.33 is about five times of magnitude higher than that of electrospun fibers with SPANI/PEO at 0.2. In addition, conducting composite fibers were also obtained through electro- spinning of SPANI/PEO solution containing different contents of c-MWCNTs. HRTEM images confirmed that the c-MWCNTs were encapsulated within the fibers as individual elements, mostly aligned along the fiber axis. The measured results showed that the electrical conductivity of the electrospun fiber mats improved with increasing the content of c-MWCNTs.
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